Development of a novel comprehensive analytical method for volatile compounds using supercritical fluid chromatography/mass spectrometry with a highly cross-linked styrene divinylbenzene polymer-based column
Development of a novel comprehensive analytical method for volatile compounds using supercritical fluid chromatography/mass spectrometry with a highly cross-linked styrene divinylbenzene polymer-based column
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采用基于高度交联苯乙烯二乙烯基苯聚合物的超临界流体色谱/质谱色谱柱开发挥发性化合物的新型综合分析方法
DOI：
10.1016/j.chroma.2020.461363
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发表时间：
2020
期刊：
影响因子：
--
通讯作者：
T.
中科院分区：
文献类型：
--
作者：
Fujito;Y.;Hayakawa;Y.;Bamba;T.
由于挥发性化合物在工业中的广泛应用，其化学性质非常多样，因此对挥发性化合物如香精、香料和香料的分析技术的需求很高。超临界流体色谱（SFC）能够高速、高高峰容量分离并且具有高分离覆盖率。由于其独特的移动的相条件，其对于制备纯化也是有利的。然而，没有可商购的用于SFC的柱适合于全面分离挥发性化合物。由于弱保留和聚合物基柱问题，如压力、溶胀和收缩公差，SFC仅限于使用硅基柱。本研究采用一种新开发的高交联苯乙烯-二乙烯基苯（SDVB）聚合物色谱柱，建立了一种适用于超临界流体中挥发性物质的综合分析方法。新开发的SDVB柱显示，与传统的硅胶柱（k > 0.3）相比，在SFC移动的条件下，具有优异的整体保留率（k > 1.6）。它还能够保留酯（羟基乙酸酯，丁酸戊酯，水杨酸甲酯）和非极性萜烯（柠檬烯，蒎烯），没有显示出足够的保留在任何其他市售的二氧化硅基柱。醛类化合物在NH_2柱上由于席夫碱的生成而发生反应，也被成功洗脱。结果表明，SDVB柱对挥发性化合物的分离全面，覆盖范围广。
Analytical techniques to determine volatile compounds such as flavor, aroma, and fragrances are in high demand due to their wide range of applications in industry, the chemical properties of them are very diverse. Supercritical fluid chromatography (SFC) is capable of high speed, high peak capacity separation and has a high separation coverage. It is also an advantageous for preparative purifications due to its unique mobile phase conditions. However, there is no column commercially available for SFC that is suitable to comprehensively separate volatile compounds. SFC is limited to the use of silica-based columns due to weak retentions and polymer-based column issues such as pressure, swelling and shrinkage tolerances. This study demonstrated comprehensive analytical method for volatile in SFC using a highly cross-linked styrene divinylbenzene (SDVB) polymer-based column, newly developed for SFC. In this study, 23 typical volatile compounds with a wide variety of chemical properties were selected as model compounds. The newly developed SDVB column showed, compared to conventional silica-based columns (k > 0.3), an excellent overall and substantial improved retentions (k > 1.6) under SFC mobile phase conditions. It was also able to retain esters (hydroxy acetate, pentyl butylate, methyl salicylate) and non-polar terpenes (limonene, pinene) that did not show sufficient retention in any other commercially available silica-based columns. Aldehydes reacting on NH2column due to Schiff base formation were also successfully eluted. It was confirmed that SDVB column provided comprehensive separation and wide coverage for volatile compounds.